CN102383030A - Preparation process for nano strengthened wear-resistant die steel - Google Patents
Preparation process for nano strengthened wear-resistant die steel Download PDFInfo
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Abstract
The invention relates to a preparation process for nano strengthened wear-resistant die steel, which comprises the steps of pre-dispersing and mixing in-situ synthesized TiB2/Al2O3 nano mixed powders and pre-dispersed iron powders in a stirring ball mill; then making into dispersed preform and adding into a steel ladle; in-situ synthesizing TiB2 nano particles and Al2O3 nano mixed powders in molten steel through high-temperature molten steel; and uniformly dispersing in a die steel base body through an electromagnetic stirrer and forming by adopting a casting process. The nano particles are in-situ synthesized, so that the wettability of the nano particles and the base body is improved, the die steel with uniformly distributed nano particles can be obtained through a secondary dispersing and electromagnetic stirring process, and the die steel is modified and strengthened. The volume fraction of the nano particles can be adjusted by adjusting the adding amount, so as to meet the requirements of different working conditions. The nano modified wear-resistant die steel has excellent mechanical property, simple production process and low preparation cost.
Description
Technical field
The invention belongs to the die steel technical field, relate to a kind of nano-powder reinforced die steels preparation method, the wear-resisting die steel preparation technology of particularly a kind of nano reinforcement.
Background technology
Development along with modern machinery and equipment and manufacturing technology; Performance and quality to part have proposed increasingly high and more and more harsher performance demands; The conventional molds steel is through in smelting molten steel, adding the alloying element of some amount, making its primary carbide that in process of setting, forms some amount, and make it separate out the proeutectoid carbide of some amount again through thermal treatment; Thereby make material keep reaching wear resistance on certain flexible basis.But owing to receive the restriction of ME; The total amount of its carbide is generally less than 20%; Because the content of carbide is less relatively; Thereby the wear resisting property of material can't satisfy the requirement of modern industry to the material abrasion resistance, and the material that promptly requires that more can't satisfy under abominable industrial and mineral working conditions has high-wearing feature, possesses the harsh requirement of multinomial performances such as HS, H.T. utmost point erosion resistance again.Therefore research and develop high-performance, high life die steel not only has good economic benefit, but also has important science and social effect.
A particulate reinforced metal-based nano composite material is exactly that nano particle is fused in metallic matrix, and nanoparticle and metallic matrix are combined closely, and makes it to have secular stability.And after compound, also can demonstrate bigger advantage at aspects such as optics, mechanical propertys.Carry out nano material and metallic matrix organically compound, the effect of utilizing the interaction of nano material and matrix to produce can also realize both mutual supplement with each other's advantages, the new functional materials of exploitation excellent performance.Experiment shows: in steel, add nonmetal nano powder, can roll up heterogeneous core external in the molten steel, make the inclusion disperseization in the steel, reduce or eliminate the deleterious effect of inclusion, so just can reduce the requirement to the steel purity.Add the also matrix of possible refinement steel of nonmetal nano powder in the steel, the existence of a large amount of heterogeneous particles can play dispersion-strengthened in steel.Therefore, in steel, add the performance that nonmetal nano powder can improve steel greatly, improve the quality of steel.Have that mechanical property is good, shearing resistance is high, working temperature is higher, wear-resistant, conductive and heat-conductive good, non-hygroscopic, not air-breathing, dimensional stabilizing, advantage such as aging, so with its excellent performance applications in robotization, space flight, aviation and high-tech sectors such as automotive industry, advanced manufacturing industry.
Because above-mentioned each item premium properties that metal-base nanometer composite material had and the extensive market prospects that is had, R and D are energetically all being carried out to it in countries in the world, and have developed various preparation technologies.At present; The method of being developed both at home and abroad for preparing metal-base nanometer composite material mainly contains mechanical alloying method (Mechanical alloying; MA), melt-spinning (Meltspun; MS) method, powder metallurgic method (Powder metallurgy; PM), machinery bring out self propagating high temperature synthetic (Self-propagatinghigh-temperature synthesis, SHS) reaction method, vacuum-evaporation inert gases agglomeration and vacuum add in-place platen press (Inert gas con-densation method combined with vacuum co-evaporation andin-situ compaction, ICVCSC) etc.; They differ from one another above-mentioned various preparation technology; The scope of application is not quite similar, and the prepared various metal-base nanometer composite materials that go out are compared all with traditional material on performance and are greatly improved, and are playing huge pushing effect aspect development conventional composite materials and the development of new matrix material.But all there is self limitation in these technologies of preparing, and wherein great majority are because apparatus expensive, complex process and be difficult to control and still concentrate on the laboratory study stage.
For realizing the manufacturing of nano particle reinforced composite, all carried out a large amount of research and developments both at home and abroad, constantly worked out new preparation technology; Making on the non-ferrous metal nano particle reinforced composite technology, Chinese invention patent ZL200510011568.4 discloses a kind of nano particle and has strengthened high-toughness casting magnesiumalloy and preparation moulding process thereof, and the magnesium alloy substrate component of this technology manufacturing and weight percent content are 5.0～10.0%Al; 0.1～1.0%Zn, 0.05～0.5%Mn, constraint element Si≤0.05%; Fe≤0.005%; Cu≤0.01%, Ni≤0.002%, all the other are magnesium.The particle that uses is the SiC nano particle, and particle diameter is less than 100nm, and addition is 0.1～3.0% of an alloy volume content.The SiC nano particle will carry out pre-treatment before adding, and its pretreatment technology is:
1, in container, import an amount of analytical pure ethanol, a certain amount of dry SiC nano particle is put into container, stir, fully wetting, SiC nano particle and alcoholic acid ratio are 1g/10ml～1g/3ml;
The polyvinyl alcohol solution that 2, will account for said mixture volume 1/50～1/10 joins in SiC nano particle and the alcoholic acid mixture, fully stirs, and mixes;
The said mixture that 3, will contain the SiC nano particle places baking oven dry, and storing temperature is 80～95 ℃.
The preparation moulding process that nano particle strengthens cast magnesium alloys is:
1, magnesium alloy materials is joined in the dry crucible of brushing coating,, use solvent or high-purity argon gas to protect, dissolve the back solution temperature and remain on 680～720 ℃ for preventing magnesium alloy from oxidative combustion in the fusion process;
2, control magnesiumalloy solution temperature to 650～700 ℃ (being higher than 60～80 ℃ of liquid magnesium alloy phase lines) or 5850～610 ℃ (being lower than 50～30 ℃ of liquid magnesium alloy phase lines); Remove surface scum; The SiC nano particle that passes through liquor treating process that accounts for magnesiumalloy volume 0.1～3.0 is added in the alloy liquid; Be pressed under the liquid level and stir churning time 3～10 minutes, 10000～2000 rev/mins of agitator speeds;
3, after the refining degasification, the control teeming temperature is 650～700 ℃ and removes out surface scum, obtains nano particle enhanced high-toughness casting Mg alloy castings through gravity mold casting or die casting.This technology through adding the nano reinforcement particle, improves the obdurability of cast magnesium alloys on the basis of traditional cast magnesium alloy; Through nano particle is carried out pre-treatment, increase the wettability of particle and magnesiumalloy:, nano particle is evenly distributed in liquid magnesium alloy through controlling suitable liquid magnesium alloy temperature and mechanical stirring technology.But because the employed SiC nano particle of this technology just can decompose at 800 ℃, and along with the rising of temperature, decomposition becomes more violent; And the SiC nano particle directly adds in the alloy; Can't solve the reunion of nano particle, the enhanced granule amount is few, uses mechanical stirring; Therefore this technology is only applicable to non-ferrous metal, and inapplicable and hot metal.Chinese invention patent ZL200510127307.9 discloses a kind of composite material with nano silicon carbide granulate strengthening aluminium base and preparation method, and this method is to adopt nano silicon carbide granulate and aluminium powder to process as raw material; Wherein the volume of nano silicon carbide granulate accounts for 0.5～20% of raw material volume, and the volume of aluminium powder accounts for 80～99.5% of raw material volume.Its preparation method is: 1, charge into argon gas again and carry out repeatedly 2～10 times vacuumizing behind the raw materials mix input sealing ball grinder; 2, high-energy ball milling; 3, hot pressed sintering; 4, hot extrusion promptly obtains composite material with nano silicon carbide granulate strengthening aluminium base.Preparation technology of the present invention is simple, and cost is low, and nano silicon carbide granulate is evenly distributed in aluminum substrate, and the powder process rate is high, and the mechanical property of matrix material is significantly increased.It has solved, and the nano level enhanced granule can not be uniformly distributed in the aluminum substrate in the method for traditional preparation process particle enhanced aluminum-based composite material, and preparation technology is numerous and diverse, the problem that cost is high.But because this process using aluminium powder is made raw material, and hot extrusion again behind the employing powder metallurgical technique hot pressed sintering, because complex process, cost is high, and facility investment is big, and technical difficulty is big, is only applicable to low-temperature metal equally.
For realizing the production of nano alloyed steel, make it on moulding stock and high-abrasive material field, realize using, in recent years, carried out a large amount of research both at home and abroad, developed some novel preparation process.Chinese invention patent ZL200610046063.6 discloses a kind of high-strength abrasion-proof thermostable nano alloyed steel material and preparation method thereof, and this invention is for to produce nano alloyed steel according to smelting process.The chemical ingredients of this material (by weight percentage) is: tungsten (W) 0.06～6.0%, manganese (Mn) 0.6～3.0%, vanadium (V) 0.06～6.0%; Niobium (Nb) 0.22～4.0%, aluminium (Mo) 0.0～7.0, carbon (C) 0.5～4.0; Chromium (Cr) 1.0～8.0, other elements 0.1～3.0, all the other are iron (Fe).Used main equipment is a vacuum induction furnace.Technical process mainly comprises the raw material preparation, goes into three process such as stove smelting, casting.Raw material adopts the pig iron or straight carbon steel, and alloy adopts the iron alloy of above-mentioned institute formulated component element.Production technique is for to carry out vacuum metling with above-mentioned various raw materials in vacuum induction furnace, when temperature reaches 1620～1750 ℃, feed stock for blast furnace all melt and composition evenly after, smelt tapping, the ingot casting moulding.The steel ingot of being produced is through checking 80% grain fineness number less than 50nm.It is simple that this technology has production technique, low cost and other advantages.But this technology only is to utilize at present the microalloy crystal grain thinning of institute's widespread use both at home and abroad; Suppress through alloying element that the grain growth principle of steel prepares; That utilizes especially that niobium (Nb) had in the metallic crystal process can suppress recrystallize; The performance of the recrystallization temperature of raising material is made, and the steel ingot of manufacturing still belongs to the fine grained steel scope, can not be called nano alloyed steel.And this technology is the mode that combines through high cleanliness molten metal and microalloying, at the certain forming core particle of the inner formation of steel, because these particles are almost separated out in the subsolidus austenite; So the forming core to austenite itself does not have the forming core central role, promptly, can only play the pinning inhibition to the grain growth in the later stage hot procedure to the not effect of refinement as cast condition crystal grain; Thereby existing purity to require height to molten steel, the quality stability of the steel alloy of being produced is poor, lacks the pinning of the second phase particle to crystal grain; Difficult quality guarantee; Defectives such as process controllability is poor, and production process control is had relatively high expectations, and the control difficulty is big.
Because the particle diameter of nano powder is little, surface energy is high, thereby has the trend of spontaneous reunion, is difficult to its ground in medium is spread out.So how improving the dispersiveness of nano-powder in medium is the key problem in technology during nano-powder material is used.Metal nano powder is applied to powder metallurgical technique, to reduce sintering temperature and to improve the performance of metallurgy product, what at first need consider is how to make metal nano powder homodisperse problem in micron powder commonly used.In addition, the nano metal based composites the preparation process in, tend to run into the compatibility problem that strengthens between body and the metallic matrix, promptly strengthen the wettability requirement of body and metallic matrix.Simultaneously, no matter be solid phase method or liquid phase method, strengthen between body and the metallic matrix all having surface reaction, it has influence on metal-base composites performance and stability during with the high temperature application when high temperature prepares.Can from metallic matrix, direct (being original position) generate if strengthen body (particle, nano particle, whisker etc.), then above-mentioned compatibility problem can be solved preferably.Generated in-situ enhancing body combines well with the metallic matrix interface, and the thermodynamic stability of production phase is good, does not have the problems such as wetting and surface reaction that strengthen between body and the metallic matrix, and this preparation method is exactly an in-situ compositing.
Original position synthetic notion originates from in-situ crystallization and the in-situ polymerization in the process of setting, receives the generally attention of Chinese scholars as a kind of breakthrough new compounding technology.Several method at present commonly used have original position solidify from think of a way, reaction in pressure sintering, internal oxidation process method, reaction mechanical alloying technology etc.The original position synthetic technology can overcome matrix with second mutually or with strengthen body and soak into bad; Surface reaction produces brittle layer; Problems such as second phase or wild phase skewness; Thereby have great potential in development of new metal-base nanometer composite material side, but present research work is focusing more on the aluminum matrix composite, and relevant original position synthesis iron base composite study is just receiving increasing attention.Because the die steel temperature of fusion is high; After adding in the steel, nano particle exists many key factors such as homodisperse technical difficulty in steel is big; Seriously restricting the Application and Development of metal-base nanometer composite material; Cause the preparation technology of present domestic and international some metal-base nanometer composite materials of developing still to rest on the experimental phase, make present research still belong to vacancy, at least also do not form product for metal-based one nano composite material.
Therefore; To have preparation technology simple in research and development, and the nano powder modified and reinforced die steels preparation method that production cost is low is to improving die steel work-ing life; Reduce the mould manufacturing cost and use cost; Enhance productivity, practice thrift valuable alloy and energy consumption, have great scientific meaning and economic implications.
Summary of the invention
The objective of the invention is to solve deficiency of the prior art; A kind of nano-powder reinforced die steels preparation method is provided; Nano particle is added in die steel and the metal wear resistant material matrix, receive meter particle is evenly distributed in the die steel matrix metal, realize the effectively compound of nano particle and die steel material; Thereby the novel high-performance nano-powder of preparing excellent performance is strengthened high abrasion die steel; It is simple that acquisition has preparation technology, and production cost is low, the wear-resisting die steel preparation method of the nano reinforcement of good product performance.
Content of the present invention comprises: original position synthesis of nano particle technology, the wear-resisting die steel technology of preparation nano reinforcement.
Nano-powder reinforced die steels basic material of the present invention is at present domestic and international applied various hot-work die steels, cold-work die steel, plastic die steel, rapid steel, heat-resistance stainless steel, superalloy, TS, and its chemical component weight per-cent is standard type component and weight percent content or the modified version component and the weight percent content of above-mentioned various die steel, rapid steel, heat-resistance stainless steel, superalloy, TS; Institute's original position synthetic nano particle is the complex body that any two kinds and the two or more mixtinites among various carbide, nitride, boride, oxide compound or carbide, nitride, boride, the oxide compound formed; The nano particle diameter is less than 100nm, and addition is 0.1%～6% of a die steel weight percent.
Preparation technology of the present invention is:
1, original position synthesis of nano particle prefabricated section preparation technology:
With purity more than or equal to 99%; Granularity is less than the industrial Ti powder of 800 μ m; Purity is more than or equal to 99%; Granularity is less than industrial Al powder, boron carbide powder and the Graphite Powder 99 of 400 μ m, and configuration proportion is that the mol ratio of B4C: Ti: Al: C is 2: (40.2～13.4): (13.5～3.7): (20.43～3.9), and to add granularity according to 5%～10 of above-mentioned powder gross weight be the Al of 300nm
2O
3, to promote the nanometer of powder, shorten the time of nanometer, improve grinding efficiency, play the effect of rapid nanoization.To pack on the high-energy stirring ball mill machine behind ball milling 20h～40h according to the original position synthesis of nano particulate material that aforementioned proportion prepares, be prepared into grain fineness number less than the synthetic TiB of the original position of 100nm
2/ Al
2O
3The nanometer mixed powder; With the synthetic TiB of the made original position of getting ready
2/ Al
2O
3The granularity that nanometer mixed powder and prediffusion are used is that 100～400 purpose iron powders take by weighing according to 1: 0.5～1: 2 ratio of weight percent; After putting into agitating ball mill and mixing; The Z 150PH dilute solution that accounts for said mixture volume 1/30～1/10 is joined in the ball mill; Fully stir, mix, pour out after processing the pre-dispersed powder of original position synthesis of nano particle; Place baking oven dry the prediffusion original position synthesis of nano particulate mixed powder that contains after mixing through 70 ℃～100 ℃ temperature baking;
2, reinforced by nanoparticles is disperseed prefabricated section preparation technology:
A, will pass through the above-mentioned pretreated original position synthesis of nano mixed powder that contains the prediffusion iron powder: borax: yellow soda ash: ammonium chloride is 100: 1: 0.5 according to nano particle mixed powder weight percent: 0.5 ratio preparation also stirs;
B, process block or granular blank with mould the original position synthesis of nano particle mixed powder that stirs, the made block or granular blank of getting ready is promptly obtained prediffusion nano-powder compound prefabricated section through 100 ℃～380 ℃ oven dry;
3, the preparation molding process of the wear-resisting die steel of nano reinforcement is:
A, employing casting production process; After said original position synthesis of nano powder compound prefabricated section taken by weighing by 0.1%～6% add-on of die steel molten steel weight; Place it in the bottom of ladle; With the die steel of required composition according to smelting technology require to smelt with refining after pour the ladle of putting into nano-powder compound prefabricated section into, the nano-powder compound prefabricated section at the bottom of high-temperature molten steel and the ladle reacts, prefabricated section original position in molten steel is synthesized TiB
2/ Al
2O
3The nanometer composite grain; Ladle called in carried out induction stirring in the magnetic stirrer about 5～15 minutes; Through adjustment and control electromagnetic agitation intensity, make original position synthesis of nano powder compound prefabricated section in molten steel, disperse the back to form fully diffusion, be evenly distributed in the die steel molten steel;
B: casting
To spread has original position to synthesize TiB
2/ Al
2O
3The die steel molten steel of nanometer composite grain carries out permanent mold casting, sand mold casting, vacuum full mold casting, rotary casting, vacuum casting moulding according to conventional die steel cast shaping process; Promptly obtain nano modification die steel casting ingot, will contain TiB according to conventional complete processing
2/ Al
2O
3The die steel casting ingot that the nanometer mixed powder is strengthened carries out electroslag casting or forging molding, manufactures the wear-resisting die steel of nano reinforcement of required geometrical shape and size.
Beneficial effect
Compared with present technology, the present invention produces effect and is embodied in:
1, the present invention adds an amount of iron powder with original position synthesis of nano particle to carry out pre-dispersed; Add an amount of sticker and flux then and process the dispersion prefabricated section; Add in the ladle; Adopt the block dispersion method that nano particle is diffused in the die steel matrix, make it in the die steel matrix, form homodisperse, adopt the casting moulding through magnetic stirrer.This process using original position synthesis of nano particle process improving the wettability of nano particle and die steel matrix, it is pollution-free to strengthen the surface, and consistency is good between matrix, interface bond strength is high; Saved that the enhancing body is synthetic separately, operations such as processing and adding, therefore, its technology is simple, cost is relatively low.
2, owing to add Al
2O
3The nanometer wild phase has promoted the nanometer of powder, shortens the time of nanometer, improves grinding efficiency, plays the effect of rapid nanoization.Simultaneously, can stop TiB effectively
2The grain growth of nano particle in high-temperature molten steel.
3, solved the difficult problem of nanoparticle agglomerates through prediffused technique; And increased the dispersity of nano particle in matrix; Obtain the die steel of uniform distribution nano particle through secondary diffusion technique and induction stirring technology, make die steel obtain modification and reinforcement.Its volume(tric)fraction of add-on adjustable through the adjustment nano particle; Guaranteeing under the material impact flexible prerequisite; Nano particle volume integral number is big more, and material wear ability is high more, in addition because the adding of nano particle can obtain heterogeneous forming core; Refinement carbide grain, the also corresponding wear resistance that improves material.
4, on the basis of traditional moulds steel and metal wear resistant material casting,, improve die steel material intensity, obdurability and wear resisting property through adding the nano reinforcement particle.
5, on diffusion technique,, make distribution and the strengthening effect of nano particle in the die steel material molten metal more effective through control proper metal liquid temp and induction stirring technology.
6, nano powder modified die steel of the present invention has good mechanical property; Can satisfy the request for utilization under the various operating modes, greatly reduce the preparation cost of nano particle enhancing modified die steel, production technique is simple; Need not specific installation, conventional cast factory can produce.
Embodiment
Embodiment 1
At Cr
12Add nano particle in the MoV cold-work die steel and carry out modification.Cr
12The chemical ingredients of MoV cold-work die steel is C1.45～1.70, Cr4.75～5.5, and Mo0.40～0.60, Si＜0.40, V0.15～0.30, Mn＜0.40, weight is 1000kg.TiB
2/ Al
2O
3Nanoparticle size is 100nm, and the add-on weight percent is 1.5%.Preparation technology is:
1) original position synthesis of nano particle prefabricated section preparation technology:
With purity more than or equal to 99%; Granularity is less than the industrial Ti powder of 800 μ m; Purity is more than or equal to 99%; Granularity is less than industrial Al powder, boron carbide powder and the Graphite Powder 99 of 400 μ m, and the mol ratio of B4C: Ti: Al: C is 2: (40.2～13.4): (13.5～3.7): (20.43～3.9), and to add granularity according to 5% of above-mentioned powder gross weight be the Al of 300nm
2O
3, to promote the nanometer of powder, shorten the time of nanometer, improve grinding efficiency, play the effect of rapid nanoization.Will according to the aforementioned proportion proportioning good original position synthesis of nano particulate material pack on the high-energy stirring ball mill machine behind ball milling 20h～40h, be prepared into the TiB of grain fineness number less than 100nm
2/ Al
2O
3The nanometer mixed powder; With the synthetic TiB of the made original position of getting ready
2/ Al
2O
3The granularity that nanometer mixed powder and prediffusion are used is that 100～400 purpose iron powders take by weighing according to 1: 0.8 ratio of weight percent; After putting into agitating ball mill and mixing; The Z 150PH dilute solution that accounts for said mixture volume 1/10 is joined in the ball mill; Fully stir, mix, pour out after processing the pre-dispersed powder of original position synthesis of nano particle; Place baking oven dry the prediffusion original position synthesis of nano particulate mixed powder that contains after mixing through 70 ℃～100 ℃ temperature baking;
2) nanoparticulate dispersed prefabricated section preparation technology:
A, will pass through the above-mentioned pretreated original position synthesis of nano mixed powder that contains the prediffusion iron powder: borax: yellow soda ash: ammonium chloride is 100: 1: 0.5 according to nano particle mixed powder weight percent: 0.5 ratio preparation also stirs;
B, process block or granular blank with mould the nano particle mixed powder that stirs, the made block or granular blank of getting ready is promptly obtained prediffusion nano-powder compound prefabricated section through 100 ℃～380 ℃ oven dry;
3) the preparation molding process of nano modification high abrasion die steel is:
A, employing permanent mold casting production technique are pressed Cr with said nano-powder compound prefabricated section
12After 1.6% add-on of MoV cold-work die steel molten steel weight takes by weighing, place it in the bottom of ladle, according to Cr
12MoV cold-work die composition of steel requires and smelting technology requires to smelt with molten steel after refining to pour the ladle of putting into original position synthesis of nano powder compound prefabricated section into; Original position synthesis of nano powder compound prefabricated section at the bottom of high-temperature molten steel and the ladle reacts, the synthetic TiB of prefabricated section original position in molten steel
2/ Al
2O
3The nanometer composite grain is called in ladle and was carried out induction stirring in the magnetic stirrer about 6 minutes, makes nano-powder compound prefabricated section in molten steel, disperse the back to form fully diffusion, is evenly distributed on Cr
12In the MoV cold-work die steel molten steel;
With spreading the Cr that nano particle is arranged
12MoV cold-work die steel molten steel pours into casting in the metal mold, promptly obtains nano powder modified Cr
12MoV cold-work die steel casting ingot; To the nano powder modified Cr after the moulding
12MoV cold-work die steel casting ingot carries out electroslag casting and forging molding processing according to conventional complete processing, manufactures the wear-resisting Cr of nano reinforcement of required geometrical shape and size
12The MoV cold-work die steel.
Embodiment 2
In the H13 hot-work die steel, add nano particle and carry out modification.The chemical ingredients of H13 hot-work die steel is C 0.31～0.45, Cr4.75～5.5, and Mo1.10～1.75, Si0.81～1.20, V0.80～1.20, Mn＜0.40, weight is 1000kg.TiB
2/ Al
2O
3Nanoparticle size is 50nm, and the add-on weight percent is 2.5%.Preparation technology is:
1) original position synthesis of nano particle prefabricated section preparation technology:
With purity more than or equal to 99%; Granularity is less than the industrial Ti powder of 800 μ m; Purity is more than or equal to 99%; Granularity is less than industrial Al powder, boron carbide powder and the Graphite Powder 99 of 400 μ m, and the mol ratio of B4C: Ti: Al: C is 2: (40.2～13.4): (13.5～3.7): (20.43～3.9), and to add granularity according to 8% of above-mentioned powder gross weight be the Al of 300nm
2O
3, to promote the nanometer of powder, shorten the time of nanometer, improve grinding efficiency, play the effect of rapid nanoization.Will according to the aforementioned proportion proportioning good original position synthesis of nano particulate material pack on the high-energy stirring ball mill machine behind ball milling 20h～40h, be prepared into the TiB of grain fineness number less than 100nm
2/ Al
2O
3The nanometer mixed powder; With the synthetic TiB of the made original position of getting ready
2/ Al
2O
3The granularity that nanometer mixed powder and prediffusion are used is that 100～400 purpose iron powders take by weighing according to 1: 1 ratio of weight percent; After putting into agitating ball mill and mixing; The Z 150PH dilute solution that accounts for said mixture volume 1/10 is joined in the ball mill; Fully stir, mix, pour out after processing the pre-dispersed powder of original position synthesis of nano particle; Place baking oven dry the prediffusion original position synthesis of nano particulate mixed powder that contains after mixing through 70 ℃～100 ℃ temperature baking;
2) nanoparticulate dispersed prefabricated section preparation technology:
A, will pass through the above-mentioned pretreated original position synthesis of nano mixed powder that contains the prediffusion iron powder: borax: yellow soda ash: ammonium chloride is 100: 1: 0.5 according to nano particle mixed powder weight percent: 0.5 ratio preparation also stirs;
B, process block or granular blank with mould the nano particle mixed powder that stirs, the made block or granular blank of getting ready is promptly obtained prediffusion nano-powder compound prefabricated section through i00 ℃～380 ℃ oven dry;
3) the preparation molding process of the wear-resisting die steel of nano reinforcement is:
A, employing permanent mold casting production technique; After said nano-powder compound prefabricated section taken by weighing by 1.6% add-on of H13 hot-work die steel molten steel weight; Place it in the bottom of ladle; Require to smelt to pour the ladle of putting into original position synthesis of nano powder compound prefabricated section into according to requirement of H13 hot-work die composition of steel and smelting technology with molten steel after refining; Original position synthesis of nano powder compound prefabricated section at the bottom of high-temperature molten steel and the ladle reacts, the synthetic TiB of prefabricated section original position in molten steel
2/ Al
2O
3The nanometer composite grain is called in ladle and is carried out induction stirring in the magnetic stirrer, makes nano-powder compound prefabricated section in molten steel, disperse the back to form fully diffusion, is evenly distributed in the H13 hot-work die steel molten steel.
Be that with the difference of embodiment the time of carrying out induction stirring is about 8 minutes.Other technological process and embodiment 1 omit together.
Embodiment 3
At W
6Mo
5Cr
4V
2Adding nano particle in the rapid steel carries out modified and reinforced.W
6Mo
5Cr
4V
2The chemical ingredients of rapid steel is C0.80～0.90, Cr3.80～4.40, and W4.50～5.50, Mo5.50～6.75, Si＜0.40, Mn＜0.40, V1.75～2.25, weight is 1000kg.TiB
2/ Al
2O
3Nanoparticle size is 70nm, and the add-on weight percent is 0.7%.
1) original position synthesis of nano particle prefabricated section preparation technology:
With purity more than or equal to 99%; Granularity is less than the industrial Ti powder of 800 μ m; Purity is more than or equal to 99%; Granularity is less than industrial Al powder, boron carbide powder and the Graphite Powder 99 of 400 μ m, and the mol ratio of B4C: Ti: Al: C is 2: (40.2～13.4): (13.5～3.7): (20.43～3.9), and to add granularity according to 8% of above-mentioned powder gross weight be the Al of 300nm
2O
3, to promote the nanometer of powder, shorten the time of nanometer, improve grinding efficiency, play the effect of rapid nanoization.Will according to the aforementioned proportion proportioning good original position synthesis of nano particulate material pack on the high-energy stirring ball mill machine behind ball milling 20h～40h, be prepared into the TiB of grain fineness number less than 100nm
2/ Al
2O
3The nanometer mixed powder; With the synthetic TiB of the made original position of getting ready
2/ Al
2O
3The granularity that nanometer mixed powder and prediffusion are used is that 100～400 purpose iron powders take by weighing according to 1: 1.5 ratio of weight percent; After putting into agitating ball mill and mixing; The Z 150PH dilute solution that accounts for said mixture volume 1/10 is joined in the ball mill; Fully stir, mix, pour out after processing the pre-dispersed powder of original position synthesis of nano particle; Place baking oven dry the prediffusion original position synthesis of nano particulate mixed powder that contains after mixing through 70 ℃～100 ℃ temperature baking;
2) nanoparticulate dispersed prefabricated section preparation technology:
A, will pass through the above-mentioned pretreated original position synthesis of nano mixed powder that contains the prediffusion iron powder: borax: yellow soda ash: ammonium chloride is 100: 1: 0.5 according to nano particle mixed powder weight percent: 0.5 ratio preparation also stirs;
B, process block or granular blank with mould the nano particle mixed powder that stirs, the made block or granular blank of getting ready is promptly obtained prediffusion nano-powder compound prefabricated section through 100 ℃～380 ℃ oven dry;
3) the preparation molding process of the wear-resisting die steel of nano reinforcement is:
A, employing permanent mold casting production technique are pressed W with said nano-powder compound prefabricated section
6Mo
5Cr
4V
2After 1.6% add-on of rapid steel molten steel weight takes by weighing, place it in the bottom of ladle, according to W
6Mo
5Cr
4V
2The rapid steel composition requires and smelting technology requires to smelt with molten steel after refining to pour the ladle of putting into original position synthesis of nano powder compound prefabricated section into; Original position synthesis of nano powder compound prefabricated section at the bottom of high-temperature molten steel and the ladle reacts, the synthetic TiB of prefabricated section original position in molten steel
2/ Al
2O
3The nanometer composite grain is called in ladle and is carried out induction stirring in the magnetic stirrer, makes nano-powder compound prefabricated section in molten steel, disperse the back to form fully diffusion, is evenly distributed on W
6Mo
5Cr
4V
2In the rapid steel molten steel.
Be that with the difference of embodiment the time of carrying out induction stirring is about 12 minutes.
Other technological process and embodiment 1,2 omit together.
Claims (2)
1. wear-resisting die steel preparation technology of nano reinforcement, its preparation technology and step are following:
(1) original position synthesis of nano particle prefabricated section preparation technology:
With purity more than or equal to 99%; Granularity is less than the industrial Ti powder of 800 μ m; Purity is more than or equal to 99%; Granularity is less than industrial Al powder, boron carbide powder and the Graphite Powder 99 of 400 μ m, and configuration proportion is that the mol ratio of B4C: Ti: Al: C is 2: (40.2～13.4): (13.5～3.7): (20.43～3.9), and to add granularity according to 5%～10 of above-mentioned powder gross weight be the Al of 300nm
2O
3To pack on the high-energy stirring ball mill machine behind ball milling 20h～40h according to the original position synthesis of nano particulate material that aforementioned proportion prepares, be prepared into grain fineness number less than the synthetic TiB of the original position of 100nm
2/ Al
2O
3The nanometer mixed powder; With the synthetic TiB of the made original position of getting ready
2/ Al
2O
3The granularity that nanometer mixed powder and prediffusion are used is that 100～400 purpose iron powders take by weighing according to 1: 0.5～1: 2 ratio of weight percent; After putting into agitating ball mill and mixing; The Z 150PH dilute solution that accounts for said mixture volume 1/30～1/10 is joined in the ball mill; Fully stir, mix, pour out after processing the pre-dispersed powder of original position synthesis of nano particle; Place baking oven dry the prediffusion original position synthesis of nano particulate mixed powder that contains after mixing through 70 ℃～100 ℃ temperature baking;
(2) nanoparticulate dispersed prefabricated section preparation technology:
A, will pass through the above-mentioned pretreated original position synthesis of nano mixed powder that contains the prediffusion iron powder: borax: yellow soda ash: ammonium chloride is 100: 1: 0.5 according to nano particle mixed powder weight percent: 0.5 ratio preparation also stirs;
B, process block or granular blank with mould the original position synthesis of nano particle mixed powder that stirs, the made block or granular blank of getting ready is promptly obtained prediffusion nano-powder compound prefabricated section through 100 ℃～380 ℃ oven dry;
(3) the preparation molding process of the wear-resisting die steel of nano reinforcement is:
A, employing casting production process; After said original position synthesis of nano powder compound prefabricated section taken by weighing by 0.1%～6% add-on of die steel molten steel weight; Place it in the bottom of ladle; With the die steel of required composition according to smelting technology require to smelt with refining after pour the ladle of putting into nano-powder compound prefabricated section into, the nano-powder compound prefabricated section at the bottom of high-temperature molten steel and the ladle reacts, prefabricated section original position in molten steel is synthesized TiB
2/ Al
2O
3The nanometer composite grain; Ladle called in carried out induction stirring in the magnetic stirrer about 5～15 minutes; Through adjustment and control electromagnetic agitation intensity, make original position synthesis of nano powder compound prefabricated section in molten steel, disperse the back to form fully diffusion, be evenly distributed in the die steel molten steel;
B: casting
To spread has original position to synthesize TiB
2/ Al
2O
3The die steel molten steel of nanometer composite grain carries out permanent mold casting, sand mold casting, vacuum full mold casting, rotary casting, vacuum casting moulding according to conventional die steel cast shaping process; Promptly obtain nano modification die steel casting ingot, will contain TiB according to conventional complete processing
2/ Al
2O
3The die steel casting ingot of nanometer mixed powder modification carries out electroslag casting or forging molding, manufactures the wear-resisting die steel of nano reinforcement of required geometrical shape and size.
2. the wear-resisting die steel of nano reinforcement according to claim 1; It is characterized in that: nano reinforcement die steel basic material is various hot-work die steels, cold-work die steel, plastic die steel, rapid steel, heat-resistance stainless steel, superalloy, TS, and its chemical component weight per-cent is standard type component and weight percent content or the modified version component and the weight percent content of above-mentioned various die steel, rapid steel, heat-resistance stainless steel, superalloy, tool steel material.
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Application publication date: 20120321 |